َ A novel conducting poly (p-nitroaniline-co-N-methylaniline) (P(p-NAn-co-NMAn)) material, obtained by electrocopolymerization of para-nitroaniline (p-NAn) and N-methylaniline(NMAn) in aqueous sulfuric acid solution. Electrosynthesiswas carried out using cyclic voltammetry technique with different monomer feed concentrations. Characterization of samples was carried out by in situ conductivity measurements,scanning electron microscopy (SEM), in situ UV-Vis, and FT-IR spectroscopy techniques. The cyclic voltammograms of P(p-NAn), P(NMAn)and P(p-NAn-co- NMAn) showedthat the peak potentials were located at different values and the effect of scan rate on that difference.The in situ conductivity of the p-NAn-co-NMAn increased with increasing the [p-NAn]/[NMAn] concentration ratio. Thein situ UV-Vis. spectroscopy results revealed strong absorption bands at different applied potentials and a spectroscopic behavior of copolymers intermediate between that of the homopolymers.The FT-IR spectroscopy and SEM analysis results showed the fundamental differences between the structures and morphology of the homo- and copolymers.